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Rotary Evaporators for Ethanol

Extraction
What is Ethanol Extraction?
Rotary evaporators are an important tool in laboratories around the world.
While this technique has many different applications, this post regards the
requirements of high purity ethanol and rotary evaporators for cannabinoid
and terpene extraction. When combined with advanced solvent extraction and
distillation processes, raw cannabis and crude cannabis yield shatter, THCA
crystals or THCA-rich oral formulations. Final packaging includes many
different forms of cannabis products including oils, tinctures, vaporizable
concentrates, and edibles. Generally, rotary evaporators allow one of the most
efficient and environmentally friendly ways of removing a volatile solvent from
a non-volatile sample. Because the solvent is recoverable and reusable, it
minimizes waste and also overhead expenditure.

Key Definitions
Extract
A substance made by extracting a part of a raw material, often by using a
solvent such as ethanol or water. Extracts may be sold as tinctures, absolutes
or in powder form.

Extraction
During this process, a solid is placed in a solvent to remove soluble
components. Making coffee or tea are common examples of extraction.

Distillation
In this process, a liquid or component is isolated by selective heating,
vaporization, and condensation. Distilleries use this to make spirits from a
mash mixture of fermented grains.

[1] (Labx.com, 2018)


How Does a Rotary Evaporator Work?
Also known as a “rotavap”, rotary evaporators use vacuum distillation to
evaporate solvent from raw or processed materials. Commonly, a cold finger
condenser connects a solvent trap which sits opposite of a flask on a rotator
unit. Cold water in the condenser creates a zone of cooling. The boiling flask
encourages evaporation, while the solvent trap is often cooled to discourage
evaporation, therefore, trapping volatile compounds once they have begun to
accumulate in a liquid phase.

Rotary Evaporator Vacuum Extraction


The introduction of a vacuum allows greater distillation capacity. Boiling points
and system pressure are codependent. System pressure and water
temperature is adjusted to provide the ideal boiling point temperature. As the
temperature of a bath or pressure lowers, the evaporating solvent could
exceed the condensation capacity of the evaporator, which causes “bumping”
or unnecessary solvent loss.

Cold Finger Glass Condensor


Rotary evaporators allow many configurations depending on the use. A
diagonal glass condenser is common for standard distillation of non-
volatile substances. Vertical class condensers allow solvents with higher
boiling points. For ethanol extraction with dry ice, a rotary evaporator with a
cold finger glass condenser is ideal. A coldfinger configuration is common for
the production of tinctures, yielding a thick concentrate that is considerably
pure with relatively little solvent use.

Water Bath Temperature


As a general rule of thumb, the water bath temperature is set twenty degrees
higher than the desired vapor temperature. For ethanol, the recommended
vapor temp is 15-20 degrees C.
Improper temperature configuration causes air within the rotary evaporator to
saturate with the solvent. This is a leading cause of solvent loss. Maximizing
solvent recovery requires an evaporator with a high degree of vacuum control
and integrity within the air seals and gaskets throughout the vacuum line.

Source: Training Papers


Distillation and Environment www.imlab.be
Vacuum Distillation
This process uses distillation under reduced pressure. Placing a liquid mixture
under vacuum enables the distillation process to occur at a lower temperature.
This lowers the liquid boiling point, increases the rate of distillation and
reduces exposure of temperature-sensitive components (this eliminates
unwanted degradation due to high heat exposure). A simple example of the
difference pressure makes to the boiling point: Water at sea level boils at
212°F (100°C); in Denver, CO, it boils at 203°F (95°C) due to lower
atmospheric pressure.

Ethanol Extraction
FCC grade ethanol is a superior grade solvent to extract plant material. This
can be used in a variety of vessels from reactors to barrels. A popular process
has the ethanol chilled to <-20°C (-4°F) either in a cold room or freezer and
then pumped into a container of cannabis. After a soak period, the ethanol
solution is either filtered or the plant material removed in a ‘tea bag’ fashion.

The resultant mother liquor of ethanol and extract is then concentrated by


removing the ethanol. Typical distillation apparatus used to remove the
ethanol include rotary evaporators or a vacuum distillation system. If a
jacketed vessel or jacketed filter reactor is used to cool ethanol for the
extraction process, a recirculating chiller acts as the cooling source.

[1] (Labx.com, 2018)

What is the Advantage of Rotary


Evaporation for Ethanol Extraction?
Rotary evaporators extract solvents at low temperatures with a high degree of
repeatability and efficiency. The method of action decreases the pressure
inside of the round bottom flask and increases the surface area through gentle
rotation which improves process time. Gentle agitation promotes thorough
evaporation and reduces the risk of bumping or flash boiling. The term
“bumping”, refers to when a large pocket of solvent vapor forms rapidly and
displaces the surrounding liquid.

Ethanol Winterization Process


Winterization is the process of removing waxes and lipids to create a
consumer ready product. Waxes and lipids often produce unfavorable traits
when heated and vaporized. Unless removed, consumption requires more
heat, diminishes flavor, increases residual residues, and may cause
harshness or irritation.
After winterization, the product is dissolved in ethanol and passes through
vacuum lines into an evaporation chamber and on to a rotating flask which
floats over a waterbath. The flask spins in order to create a thin film on the
wall of the flask, causing slow and controlled precipitation of any volatile
solvents.
When exposed to heat, this experiment shows that a mild water bath is
favorable over intensive heating. For ethanol extraction, dry ice within the
vertical “coldfinger” silo allows ultra-low temperatures which coax a complete
removal of residual solvents from the target product. Room temperature
evaporation often produces greater volumes of waxes and pigments. These
byproducts may produce discoloration, harshness, or less palatable flavors,
hence super-chilled extractions remain preferred.

Rotary Evaporation Temperatures


A vacuum pump lowers a solvents boiling point by reducing pressure within
the rotary evaporator. The water bath is deployed at 30-40 degrees with an
ethanol vapor temperature 15-20 degrees C. Lower water bath temperatures
prevent thermal decomposition. Increasing the evaporation rate by lowering
the vacuum and/or increasing the water bath temperature can lead to capacity
overload on the condenser. (Julabo)

Best Ethanol for Rotary Evaporator


Extraction?
FCC grade ethyl alcohol (ethanol) is a mounting standard during concentrate
extraction and food-related cannabis products. FCC approved products
designate the highest purity for consumable products with no contaminants
such as denaturants, heavy metals, methanol, hexane, and benzene. The
purest solvents allow perfectibility and more consistent yields while also
producing cleaner, better tasting concentrates.

Ethanol Flammability
Ethanol meets the criteria for a Category 2 flammable liquid, according to
OSHA’s Flammable Liquids standard and the HCS (29 CFR 1910.106; 29
CFR 1910.1200 Appendix B). This is because ethanol ignites at normal room
temperatures, has a flash point of 55°F, and has a boiling point of 173°F [2]
(OSHA/EPA, 2011).
Related Post: High-Purity Solvents for Cannabis Extraction

Rotary Evaporator Configuration


Diagrams & Images

The method of action decreases the pressure inside of the round bottom flask
and increases the surface area through gentle rotation which improves
process time. Gentle agitation promotes through evaporation and reduces the
risk of bumping or flash boiling.
Yamato Set C (use with dry ice).
The cold finger glass condenser is set vertically, suitable for distillation of
volatile or low boiling point solvents. When space is limited, the use of a
vertical condenser set up is recommended.
The water condenser is replaced by a cold trap that enables very low freezing
temperatures. Hence, with this assembly, it is also possible to completely
condense extremely volatile and low-boiling solvents such as chloroform or
dichloromethane. You can fill the cold trap not only with common freezing
mixtures such as dry ice/acetone (-70°C) or ice/common salt (-20°C) but also
with liquid nitrogen (approx. -190°C). This allows you to perform sublimations
as well. The cold trap does not require running water for cooling; therefore, it
saves water.